#------------------------------------------------------------------------------
#$Date: 2019-11-07 21:34:14 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223546 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/21/7232133.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7232133
loop_
_publ_author_name
'Chalmers, James E.'
'Srivastava, Anant Kumar'
'Dixey, Richard J. C.'
'Sivakumaran, Krrishna'
'Saines, Paul J.'
_publ_section_title
;
 Low dimensional and frustrated antiferromagnetic interactions in
 transition metal chloride complexes with simple amine ligands
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              894
_journal_paper_doi               10.1039/C8CE01901K
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C2 H10 Cl2 Cu N2 O2'
_chemical_formula_sum            'C2 H10 Cl2 Cu N2 O2'
_chemical_formula_weight         228.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-07-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-06 deposited with the CCDC.
2018-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                99.853(12)
_cell_angle_beta                 98.563(12)
_cell_angle_gamma                91.568(13)
_cell_formula_units_Z            1
_cell_length_a                   3.7868(6)
_cell_length_b                   5.6827(9)
_cell_length_c                   8.7079(11)
_cell_measurement_reflns_used    2099
_cell_measurement_temperature    150.0(4)
_cell_measurement_theta_max      75.8200
_cell_measurement_theta_min      5.1350
_cell_volume                     182.30(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2774
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -115.00 -17.00   1.00    4.00    --  -41.22 -38.00 -60.00   98
  2  ω   -115.00 -17.00   1.00    4.00    --  -41.22 -38.00  30.00   98
  3  ω    -35.00  74.00   1.00    4.00    --   41.22 -77.00-150.00  109
  4  ω     23.00  97.00   1.00    4.00    --   41.22-125.00-150.00   74
  5  ω     86.00 178.00   1.00    8.00    --  112.00  45.00 -90.00   92
  6  ω     29.00 109.00   1.00    8.00    --  112.00 -94.00  60.00   80
  7  ω     39.00 138.00   1.00    8.00    --  112.00 -45.00  30.00   99
  8  ω     36.00 116.00   1.00    8.00    --  112.00-111.00 -60.00   80
  9  ω    100.00 178.00   1.00    8.00    --  112.00 111.00 120.00   78
 10  ω     86.00 178.00   1.00    8.00    --  112.00  45.00-150.00   92
 11  ω    100.00 178.00   1.00    8.00    --  112.00 111.00  90.00   78
 12  ω     29.00 109.00   1.00    8.00    --  112.00 -94.00 -30.00   80
 13  ω     57.00 151.00   1.00    8.00    --  112.00 178.00 -90.00   94
 14  ω     57.00 151.00   1.00    8.00    --  112.00 178.00 -30.00   94
 15  ω     79.00 178.00   1.00    8.00    --  112.00  77.00   0.00   99
 16  ω   -113.00 -65.00   1.00    4.00    --  -41.22-138.00-112.00   48
 17  ω   -113.00 -13.00   1.00    4.00    --  -41.22 -57.00-120.00  100
 18  ω   -113.00 -13.00   1.00    4.00    --  -41.22 -57.00 150.00  100
 19  ω      9.00 117.00   1.00    4.00    --   41.22  77.00  30.00  108
 20  ω      1.00  82.00   1.00    4.00    --   41.22 -99.00 -60.00   81
 21  ω     83.00 178.00   1.00    8.00    --  112.00  61.00 150.00   95
 22  ω     79.00 178.00   1.00    8.00    --  112.00  77.00  30.00   99
 23  ω     84.00 178.00   1.00    8.00    --  112.00  30.00  90.00   94
 24  ω     79.00 178.00   1.00    8.00    --  112.00  77.00-150.00   99
 25  ω     84.00 178.00   1.00    8.00    --  112.00  30.00  60.00   94
 26  ω     84.00 178.00   1.00    8.00    --  112.00  30.00 -60.00   94
 27  ω     83.00 178.00   1.00    8.00    --  112.00  61.00-180.00   95
 28  ω     79.00 178.00   1.00    8.00    --  112.00  77.00 -30.00   99
 29  ω     86.00 178.00   1.00    8.00    --  112.00  45.00 150.00   92
 30  ω     83.00 178.00   1.00    8.00    --  112.00  61.00 -60.00   95
 31  ω     79.00 178.00   1.00    8.00    --  112.00  77.00  90.00   99
 32  ω     83.00 178.00   1.00    8.00    --  112.00  61.00-150.00   95
 33  ω     83.00 178.00   1.00    8.00    --  112.00  61.00   0.00   95
 34  ω     86.00 178.00   1.00    8.00    --  112.00  45.00  90.00   92
 35  ω     86.00 178.00   1.00    8.00    --  112.00  45.00 -30.00   92
 36  ω      1.00  82.00   1.00    4.00    --   41.22 -99.00  90.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1419345000
_diffrn_orient_matrix_UB_12      0.2435673000
_diffrn_orient_matrix_UB_13      -0.0275258000
_diffrn_orient_matrix_UB_21      0.0975195000
_diffrn_orient_matrix_UB_22      0.0839496000
_diffrn_orient_matrix_UB_23      0.1796178000
_diffrn_orient_matrix_UB_31      0.3743037000
_diffrn_orient_matrix_UB_32      -0.0977781000
_diffrn_orient_matrix_UB_33      -0.0051546000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3563
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         76.510
_diffrn_reflns_theta_min         5.219
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.472
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.082
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             115
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.151
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0539P)²+0.0338P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                715
_reflns_number_total             759
_reflns_threshold_expression     'I > 2σ(I)'
_iucr_refine_instructions_details
;

    18_pjs_019.res created by SHELXL-2014/7

TITL 18_pjs_019_a.res in P-1
REM Old TITL 18_PJS_019 in P-1 #2
REM SHELXT solution in P-1
REM R1 0.162, Rweak 0.009, Alpha 0.023, Orientation as input
REM Formula found by SHELXT: O2 Cu
CELL 1.54184 3.786793 5.68273 8.707909 99.8531 98.5632 91.5683
ZERR 1 0.000646 0.000861 0.001055 0.0115 0.012 0.013
LATT 1
SFAC Cu Cl C O N H
UNIT 1 2 2 2 2 10
 
L.S. 10
PLAN  20
SIZE 0.163 0.022 0.018
BOND $H
LIST 6
fmap 2
acta 134
REM <olex2.extras>
REM <HklSrc "%./18_PJS_019.hkl">
REM </olex2.extras>
 
WGHT    0.053900    0.033800
FVAR       1.37156
CU1   1    0.500000    0.500000    0.500000    10.50000    0.01371    0.01404 =
         0.01501    0.00545   -0.00166   -0.00208
CL1   2    0.043254    0.229866    0.366534    11.00000    0.01467    0.01529 =
         0.01747    0.00280   -0.00014   -0.00138
O1    4    0.753082    0.366639    0.812133    11.00000    0.01602    0.02377 =
         0.01655    0.00772   -0.00326   -0.00368
N1    5    0.490406    0.308884    0.672840    11.00000    0.01346    0.01864 =
         0.01436    0.00502   -0.00233   -0.00153
AFIX  23
H1A   6    0.275841    0.320539    0.702693    11.00000   -1.20000
H1B   6    0.509338    0.156128    0.631582    11.00000   -1.20000
AFIX   0
C1    3    0.671980    0.225770    0.925975    11.00000    0.01820    0.02469 =
         0.01834    0.00929    0.00204    0.00316
AFIX 137
H1C   6    0.681351    0.059088    0.883369    11.00000   -1.50000
H1D   6    0.436678    0.257254    0.950082    11.00000   -1.50000
H1E   6    0.843751    0.266898    1.020497    11.00000   -1.50000
AFIX   0
HKLF 4
 
REM  18_pjs_019_a.res in P-1
REM R1 =  0.0314 for     715 Fo > 4sig(Fo)  and  0.0331 for all     759 data
REM     44 parameters refined using      0 restraints
 
END  
     
WGHT      0.0539      0.0338 

REM Highest difference peak  1.151,  deepest hole -0.445,  1-sigma level  0.119
Q1    1   0.0000  0.5000  0.5000  10.50000  0.05    1.15
Q2    1   0.2176  0.5108  0.5055  11.00000  0.05    0.75
Q3    1   0.4639  0.7726  0.6355  11.00000  0.05    0.67
Q4    1  -0.2320  0.2576  0.3814  11.00000  0.05    0.56
Q5    1   0.2673  0.2179  0.3789  11.00000  0.05    0.48
Q6    1   0.1543  0.2632  0.5170  11.00000  0.05    0.36
Q7    1  -0.0341  0.2643  0.6151  11.00000  0.05    0.35
Q8    1   0.2239  0.3505  0.8010  11.00000  0.05    0.32
Q9    1  -0.0616  0.3895  0.4200  11.00000  0.05    0.31
Q10   1   0.3999  0.4614  0.3526  11.00000  0.05    0.31
Q11   1   0.1525  0.5172  0.4030  11.00000  0.05    0.30
Q12   1  -0.0591  0.2079  0.2471  11.00000  0.05    0.30
Q13   1   0.3469  0.1795  0.4634  11.00000  0.05    0.29
Q14   1   0.4009  0.6450  0.7189  11.00000  0.05    0.28
Q15   1   0.5000  0.0000  0.5000  10.50000  0.05    0.27
Q16   1  -0.0031  0.1534  0.2982  11.00000  0.05    0.27
Q17   1   0.8305  0.0880  0.7035  11.00000  0.05    0.26
Q18   1   0.1059  0.1018  0.4064  11.00000  0.05    0.26
Q19   1   0.8841  0.0680  0.7452  11.00000  0.05    0.25
Q20   1  -0.0178  0.2038  0.3840  11.00000  0.05    0.25

  REM The information below was added by Olex2.
  REM
  REM R1 = 0.0314 for 715 Fo > 4sig(Fo) and 0.0331 for all 3563 data
  REM n/a parameters refined using n/a restraints
  REM Highest difference peak 1.15, deepest hole -0.45
  REM Mean Shift 0, Max Shift 0.000.

  REM +++ Tabular Listing of Refinement Information +++
  REM R1_all = 0.0331
  REM R1_gt = 0.0314
  REM wR_ref = 0.0844
  REM GOOF = 1.096
  REM Shift_max = 0.000
  REM Shift_mean = 0
  REM Reflections_all = 3563
  REM Reflections_gt = 715
  REM Parameters = n/a
  REM Hole = -0.45
  REM Peak = 1.15
  REM Flack = n/a

  
;
_cod_data_source_file            c8ce01901k2.cif
_cod_data_source_block           18_pjs_019_MHA2CuCl2
_cod_depositor_comments
'Adding full bibliography for 7232129--7232133.cif.'
_cod_database_code               7232133
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Cu C O N H'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.834
_shelx_estimated_absorpt_t_min   0.280
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
2.b Idealised Me refined as rotating group:
 C1(H1C,H1D,H1E)
;
_olex2_date_sample_data_collection 2017-10-25
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.416
_oxdiff_exptl_absorpt_empirical_full_min 0.788
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu1 Cu 0.5000 0.5000 0.5000 0.0144(2) Uani 1 2 d S T P
Cl1 Cl 0.04325(13) 0.22987(8) 0.36653(5) 0.0161(2) Uani 1 1 d . . .
O1 O 0.7531(4) 0.3666(3) 0.81213(18) 0.0190(4) Uani 1 1 d . . .
N1 N 0.4904(5) 0.3089(3) 0.6728(2) 0.0157(4) Uani 1 1 d . . .
H1A H 0.2758 0.3205 0.7027 0.019 Uiso 1 1 calc R . .
H1B H 0.5093 0.1561 0.6316 0.019 Uiso 1 1 calc R . .
C1 C 0.6720(7) 0.2258(4) 0.9260(3) 0.0198(5) Uani 1 1 d . . .
H1C H 0.6814 0.0591 0.8834 0.030 Uiso 1 1 calc GR . .
H1D H 0.4367 0.2573 0.9501 0.030 Uiso 1 1 calc GR . .
H1E H 0.8438 0.2669 1.0205 0.030 Uiso 1 1 calc GR . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0137(3) 0.0140(3) 0.0150(3) 0.00545(18) -0.00166(19) -0.00208(19)
Cl1 0.0147(3) 0.0153(3) 0.0175(3) 0.0028(2) -0.0001(2) -0.0014(2)
O1 0.0160(8) 0.0238(7) 0.0165(7) 0.0077(6) -0.0033(6) -0.0037(6)
N1 0.0135(9) 0.0186(8) 0.0144(8) 0.0050(6) -0.0023(7) -0.0015(7)
C1 0.0182(11) 0.0247(10) 0.0183(10) 0.0093(8) 0.0020(8) 0.0032(9)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Cl1 Cu1 Cl1 180.0 2_666 .
N1 Cu1 Cl1 83.95(5) . .
N1 Cu1 Cl1 83.95(5) 2_666 2_666
N1 Cu1 Cl1 96.05(5) . 2_666
N1 Cu1 Cl1 96.05(5) 2_666 .
N1 Cu1 N1 180.0 2_666 .
N1 O1 C1 109.20(15) . .
Cu1 N1 H1A 107.6 . .
Cu1 N1 H1B 107.6 . .
O1 N1 Cu1 118.86(12) . .
O1 N1 H1A 107.6 . .
O1 N1 H1B 107.6 . .
H1A N1 H1B 107.0 . .
O1 C1 H1C 109.5 . .
O1 C1 H1D 109.5 . .
O1 C1 H1E 109.5 . .
H1C C1 H1D 109.5 . .
H1C C1 H1E 109.5 . .
H1D C1 H1E 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 Cl1 2.3118(6) .
Cu1 Cl1 2.3117(6) 2_666
Cu1 N1 2.0049(17) .
Cu1 N1 2.0049(17) 2_666
O1 N1 1.434(2) .
O1 C1 1.438(2) .
N1 H1A 0.8900 .
N1 H1B 0.8900 .
C1 H1C 0.9600 .
C1 H1D 0.9600 .
C1 H1E 0.9600 .
